Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tri(butyl)vinyltin → 1-(2-Methyl-4-nitrophenyl)-3-vinylpyridin-2(1H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tri(butyl)vinyltin | HCID 53438229 | — |
| 반응물 | 3-Bromo-1-(2-methyl-4-nitrophenyl)pyridin-2(1H)-one | HCID 59410157 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 1-(2-Methyl-4-nitrophenyl)-3-vinylpyridin-2(1H)-one | HCID 59410198 | — |
반응 단계
50 g (162 mmol) of the compound from example 41A are dissolved in 700 ml of anhydrous dioxane and admixed with 62 g (194 mmol) of tributylvinyltin and 4.7 g (4.0 mmol) of tetrakis(triphenylphosphine)palladium, and the mixture is heated at reflux for 15 h. It is allowed to cool and filtered through kieselguhr. It is washed with ethyl acetate, and the combined filtrates are concentrated to dryness under reduced pressure. The residue is applied to silica gel and chromatographed on 800 g of silica gel with a gradient of cyclohexane and ethyl acetate. This affords 27 g (62% of theory) of the desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08198267B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-1ce46bb10fc0475cb1a816ef8e29b722 |
| 출처 메모 | uspto-grants-2012_06 |